CN106830424B - Zero-emission treatment method and system for removing calcium and magnesium by using carbon dioxide spray reaction - Google Patents
Zero-emission treatment method and system for removing calcium and magnesium by using carbon dioxide spray reaction Download PDFInfo
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Abstract
The invention discloses a zero-emission treatment method and a zero-emission treatment system for removing calcium and magnesium by using a carbon dioxide spraying reaction. The method comprises the steps of converting calcium ions and magnesium ions into carbonate precipitates by carbon dioxide spraying of the high-calcium magnesium ion wastewater, separating the precipitates, treating supernatant containing trace carbonate precipitates by a membrane concentration unit, directly recycling pure water, and performing multi-effect evaporation treatment on the rest concentrated water; the precipitate obtained by the separation treatment is converted into sludge through filter pressing, and the sludge is transported outside; according to the invention, the carbon dioxide spraying reaction tower, the precipitation unit, the membrane concentration unit, the multiple-effect evaporation treatment unit and the filter pressing unit are organically combined, calcium and magnesium ions in the wastewater are separated and removed step by step, zero emission is really realized, and the method has good social value and market value.
Description
Technical Field
The invention belongs to the technical field of wastewater discharge, and particularly relates to a zero discharge treatment method and a zero discharge treatment system for wastewater containing high calcium and magnesium ions, high alkalinity and high salt content, in particular to a process method and a system for implementing zero discharge treatment for heavy acidic wastewater in mining industry, comprehensive terminal wastewater in thermal power plants, high alkalinity, high hardness and high salt content chemical wastewater and the like.
Background
With the development of mining industry, metallurgy and chemical industry, the generated high-salinity wastewater is difficult to treat, the treatment processes such as lime and alkali neutralization are usually adopted, the lime treatment process has a certain effect on removing heavy metal ions, but a large amount of calcium and magnesium ions are introduced in the treatment process, so that the concentration of the wastewater ions is higher and higher, and the zero discharge of the conventional water treatment process is difficult to achieve.
At present, the membrane concentration and decrement process is mainly adopted, but zero emission cannot be really realized, and the reason is that: the waste water to be treated contains a large amount of calcium and magnesium ions, a large amount of pollution and blockage phenomena are easy to occur in the membrane concentration treatment process, the membrane is irrecoverable to be damaged, and the membrane replacement frequency is high, so that the total operation cost of the process is high, and enterprises are difficult to bear.
At present, no method for zero-discharge treatment of a large amount of calcium and magnesium ions in wastewater is reported.
Disclosure of Invention
Aiming at the difficulties and problems in zero-discharge treatment of the wastewater containing high calcium and magnesium ions in the prior art, the invention aims to provide a zero-discharge treatment method for removing calcium and magnesium by utilizing carbon dioxide spray reaction.
The invention also aims to provide a zero-rank processing system based on the zero-rank processing method.
The above object of the present invention is achieved by the following means.
A zero-emission treatment method for removing calcium and magnesium by using carbon dioxide spray reaction comprises the following steps:
s1, converting calcium and magnesium ions in the wastewater containing high calcium and magnesium ions into carbonate precipitates through a carbon dioxide spraying reaction, wherein the concentration of the calcium and magnesium ions in the wastewater is 10000-12000 mg/L, the feed-liquid ratio of carbon dioxide introduced in a unit time to the wastewater is 0.6-2.4: 1 (mol/L), and precipitating and separating a mixture obtained through the spraying reaction;
s2, performing membrane concentration treatment on the separated supernatant containing trace carbonate precipitate, directly recycling the obtained pure water, and performing multi-effect evaporation treatment on the rest concentrated water;
s3, converting the precipitate obtained after the separation treatment into sludge through pressure filtration treatment, and transporting the sludge outside.
The carbon dioxide showering reaction means that carbon dioxide contacts with high calcium and magnesium ions in the showering waste water from bottom to top to fully react. The invention uses a plurality of water treatment processes in a combined way, gradually separates and removes ions in the wastewater, transports the sludge outwards and really realizes zero emission.
Preferably, the sludge obtained after the multi-effect evaporation treatment in the step S2 and the sludge in the step S3 are both subjected to outward transportation treatment.
Preferably, in the step S1, organic amine is added to the wastewater as a stabilizer, the concentration of the organic amine is 0.01 to 1mmol/L, the spraying reaction temperature is 5 to 30 ℃, and the spraying reaction pressure is 0.1 to 0.5 Mpa.
Preferably, the organic amine is diethylenetriamine or ammonia water. More preferably, the concentration of the organic amine diethylenetriamine or ammonia water is 0.6 mmol/L.
Preferably, the conditions for precipitation in step S1 are: the pH value is 7-8, the temperature is 5-30 ℃, and the deposition retention time is 30-60 min.
Preferably, the membrane concentration treatment in step S2 includes ultrafiltration pretreatment and reverse osmosis concentration treatment, the operating pressure of the ultrafiltration pretreatment is 0.1 to 0.3Mpa, and the operating pressure of the reverse osmosis concentration treatment is 0.9 to 2.5 Mpa.
Preferably, the operation pressure of the filter pressing treatment in the step S3 is 0.3-0.6 Mpa, and the water content of the sludge is 75-80%.
Preferably, in the step S1, the spray reaction employs a spray reaction tower, and the precipitation and separation process employs an inclined plate precipitation unit; in the step S2, a membrane concentration unit is adopted in the membrane concentration treatment, and a steam mechanical recompression evaporator is adopted in the multi-effect evaporation treatment; and in the step S3, a plate-and-frame filter press is adopted for filter pressing treatment.
The invention also provides a zero discharge treatment system for realizing the zero discharge treatment method for removing calcium and magnesium by using the carbon dioxide spray reaction, which comprises a carbon dioxide spray reaction tower, an inclined plate precipitation unit, a membrane concentration unit, a multi-effect evaporation unit and a filter pressing unit which are connected in sequence.
Preferably, the multiple-effect evaporation unit adopts a steam mechanical recompression evaporation unit, so that the heat utilization efficiency is high, and the energy consumption is low.
Preferably, the carbon dioxide spraying reaction tower is provided with a gas distribution device and a spraying device, and carbon dioxide enters the spraying reaction tower through the gas distribution device at the bottom; the wastewater enters a spraying reaction tower through a spraying device at the top; and the wastewater after reaction flows through a self-flowing groove in the spraying reaction tower to a tower bottom collecting tank and then enters the inclined plate sedimentation tank through self-flowing or a pump.
Preferably, the carbon dioxide tail gas which is not completely reacted is recycled and enters the spraying reaction tower again through the gas distribution device for recycling.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a zero-emission treatment method for removing calcium and magnesium by utilizing carbon dioxide spray reaction, which optimizes process parameters and realizes zero emission of wastewater through organic cooperation of various treatment technologies.
(2) The process method has the advantages of simple flow, large water treatment amount, low energy consumption, economy and environmental protection.
(3) Most of calcium and magnesium ions are removed by utilizing carbon dioxide spraying reaction, the normal operation of membrane concentration treatment is ensured, and the utilization rate of water resources is high.
(4) The invention adopts the steam mechanical recompression evaporator, has high heat utilization efficiency and low energy consumption.
Drawings
FIG. 1 is a process flow diagram of a zero-emission treatment method for removing calcium and magnesium by using carbon dioxide spray reaction according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
As shown in the figure 1, the zero-emission treatment method for removing calcium and magnesium by using carbon dioxide spray reaction comprises the following steps:
s1, converting calcium and magnesium ions in the wastewater containing high calcium and magnesium ions into carbonate precipitates through a carbon dioxide spraying reaction, wherein the concentration of the calcium and magnesium ions in the wastewater is 10000-12000 mg/L, the feed-liquid ratio of carbon dioxide introduced in a unit time to the wastewater is 0.6-2.4: 1 (mol/L), and precipitating and separating a mixture obtained through the spraying reaction;
s2, performing membrane concentration treatment on the separated supernatant containing trace carbonate precipitate, directly recycling the obtained pure water, and performing multi-effect evaporation treatment on the rest concentrated water;
s3, converting the precipitate obtained after the separation treatment into sludge through pressure filtration treatment, and transporting the sludge outside.
Wherein, carbon dioxide is used as a precipitator, and organic amine is added into the wastewater as a stabilizer, so that calcium and magnesium ions are precipitated. Carbon dioxide enters the reaction tower through the gas distribution device, and wastewater enters the reaction tower through the shower device. The carbon dioxide is contacted with the sprayed wastewater containing high calcium and magnesium ions from bottom to top to fully react, the wastewater after the reaction flows from a self-flowing groove in the tower to a collecting tank at the bottom of the tower and enters an inclined plate precipitation unit through self-flowing or a pump, and the carbon dioxide tail gas which is not completely reacted is recycled and enters the reaction tower again for recycling.
A treatment system for realizing the treatment method comprises a carbon dioxide spraying reaction tower, an inclined plate precipitation unit, a membrane concentration unit, a multi-effect evaporation unit and a filter pressing unit which are connected in sequence. Specifically, in the step S1, the spray reaction is performed by using a carbon dioxide spray reaction tower, and the precipitation and separation treatment is performed by using an inclined plate sedimentation tank; in the step S2, a membrane concentration unit is adopted in the membrane concentration treatment, and a steam mechanical recompression evaporator is adopted in the multi-effect evaporation treatment; and in the step S3, a plate-and-frame filter press is adopted for filter pressing treatment.
In a preferred embodiment, the organic amine is diethylenetriamine or ammonia water, and the concentration is 0.6 mmol/L.
The process of the present invention will be further described below by taking specific examples of the conditions for carrying out the process.
Example 1
The calcium ion concentration of the three-stage neutralization wastewater of a certain copper industry wastewater treatment station is 9600mg/L, and the magnesium concentration is 2010 mg/L.
The method for treating the wastewater comprises the following steps:
s1, converting calcium and magnesium ions of the wastewater containing high calcium and magnesium ions into carbonate precipitates through a carbon dioxide spraying reaction tower, wherein the feed-liquid ratio of introduced carbon dioxide to the wastewater in unit time is 1.5:1 (mol/L), the wastewater is also added with a stabilizer organic amine diethylenetriamine, the concentration of the organic amine diethylenetriamine is 0.01mmol/L, the temperature of the reaction tower is 10 ℃, the pressure in the reaction tower is 0.2Mpa, after treatment, calcium and magnesium ions generate calcium carbonate and magnesium carbonate precipitates under the action of a precipitator carbon dioxide and the stabilizer organic amine, a mixture is subjected to separation treatment through an inclined plate precipitation tank, the pH value in the inclined plate precipitation tank is =7.5, the temperature is 11 ℃, the precipitation residence time is 33 minutes, the concentration of calcium ions in a supernatant is 180mg/L, and the concentration of magnesium ions is 80 mg/L.
S2, pretreating the separated supernatant containing trace carbonate precipitate by an ultrafiltration membrane unit at an operating pressure of 0.2 MPa; then the pure water enters a reverse osmosis membrane unit for concentration, the operation pressure is 1.1Mpa, the yield of the pure water is more than 85 percent, and the obtained pure water is directly recycled; generating 10% of concentrated water, carrying out multi-effect evaporation treatment on the concentrated water, and converting evaporation residues into sludge;
and S3, converting the precipitate obtained in the step S1 into sludge through pressure filtration, mixing the sludge with the sludge obtained in the step S2, and transporting the sludge out, wherein the operating pressure of the pressure filtration is 0.4Mpa, and the water content of the sludge is 75%.
Example 2
The present example is substantially the same as example 1 in the treatment of wastewater containing high calcium and magnesium ions, except that: in the step S1, the feed-liquid ratio of the carbon dioxide introduced per unit time to the wastewater is 2.0:1 (mol/L).
As a result: the concentration of calcium ions in the supernatant of S1 was 120mg/L, and the concentration of magnesium ions was 75 mg/L.
Example 3
The present example is substantially the same as example 1 in the treatment of wastewater containing high calcium and magnesium ions, except that: in the step S1, the feed-liquid ratio of the carbon dioxide introduced per unit time to the wastewater is 2.2:1 (mol/L), and the concentration of the organic amine is 0.6 mmol/L.
As a result: the concentration of calcium ions in the supernatant of S1 was 90mg/L, and the concentration of magnesium ions was 60 mg/L.
Compared with treatment effects of embodiments 1-3, the treatment effect is better and better as the concentration of calcium and magnesium ions in the supernatant is reduced by increasing the feed-liquid ratio of carbon dioxide to wastewater to a certain extent and increasing the dosage of organic amine. Preferably, the organic amine is diethylenetriamine, and the concentration is 0.6 mmol/L. The preferable ratio of carbon dioxide to waste water is 2.0:1 (mol/L), and if the relative introduction amount of carbon dioxide is further increased, the effect of removing calcium and magnesium is not obviously improved.
Example 4
After desulfurization waste water of a certain thermal power plant is neutralized by lime milk, the concentration of calcium ions is 9000mg/L, and the concentration of magnesium ions is 1030 mg/L.
The method for treating the neutralized wastewater comprises the following steps:
s1, converting calcium and magnesium ions of the wastewater containing high calcium and magnesium ions into carbonate precipitates through a carbon dioxide spray reaction tower, wherein the feed-liquid ratio of carbon dioxide introduced in unit time to the wastewater is 0.6:1 (mol/L), the wastewater is also added with stabilizer organic amine ammonia water, the concentration of the organic amine is 0.6mmol/L, the temperature of the reaction tower is 12 ℃, the pressure in the reaction tower is 0.2Mpa, after treatment, the calcium and magnesium ions generate calcium carbonate and magnesium carbonate precipitates under the action of the precipitant carbon dioxide and the stabilizer organic amine, a mixture is subjected to separation treatment through an inclined plate precipitation tank, the pH =8, the temperature is 15 ℃, the precipitation residence time is 50 minutes, the calcium ion concentration of supernatant is 190mg/L, and the magnesium ion concentration is 130 mg/L.
S2, pretreating the separated supernatant containing trace carbonate precipitate by an ultrafiltration membrane unit at an operating pressure of 0.2 MPa; then the pure water enters a reverse osmosis membrane unit for concentration, the operation pressure is 1.5Mpa, the yield of the pure water is more than 85 percent, and the obtained pure water is directly recycled; generating 10% of concentrated water, carrying out multi-effect evaporation treatment on the concentrated water, and converting evaporation residues into sludge;
and S3, converting the precipitate obtained in the step S1 into sludge through pressure filtration, mixing the sludge with the sludge obtained in the step S2, and transporting the sludge out, wherein the operating pressure of the pressure filtration is 0.5Mpa, and the water content of the sludge is 75%.
Example 5
The present example is basically the same as example 4 in the treatment of wastewater containing high calcium and magnesium ions, except that: in the step S1, the feed-liquid ratio of the carbon dioxide introduced per unit time to the wastewater is 1.5:1 (mol/L).
As a result: the concentration of calcium ions in the supernatant of S1 was 170mg/L, and the concentration of magnesium ions was 120 mg/L.
Example 6
The present example is basically the same as example 4 in the treatment of wastewater containing high calcium and magnesium ions, except that: in the step S1, the feed-liquid ratio of the carbon dioxide introduced per unit time to the wastewater is 1.8:1 (mol/L), and the concentration of the organic amine is 0.4 mmol/L.
As a result: the concentration of calcium ions in the supernatant of S1 was 160mg/L, and the concentration of magnesium ions was 110 mg/L.
Compared with the treatment effects of the embodiments 4 to 6, the preferable concentration of the organic amine ammonia water is 0.6 mmol/L; and the preferable feed-liquid ratio of the carbon dioxide to the wastewater is 1.5:1 (mol/L), the concentration of calcium and magnesium ions in the supernatant is reduced, the treatment effect is obvious, and if the relative introduction amount of the carbon dioxide is further increased, the calcium and magnesium removal effect is not obviously improved.
Example 7
After acid wastewater of a certain chemical plant is neutralized by lime, the concentration of calcium ions is 11000mg/L, and the concentration of magnesium ions is 1000 mg/L.
The method for treating the neutralized wastewater comprises the following steps:
s1, converting calcium and magnesium ions of the wastewater containing high calcium and magnesium ions into carbonate precipitates through a carbon dioxide spraying reaction tower, wherein the feed-liquid ratio of introduced carbon dioxide to the wastewater in unit time is 2.4:1 (mol/L), the wastewater is also added with a stabilizer organic amine diethylenetriamine, the concentration of the organic amine is 0.1mmol/L, the temperature of the reaction tower is 25 ℃, the pressure in the reaction tower is 0.3Mpa, after treatment, the calcium and magnesium ions generate calcium carbonate and magnesium carbonate precipitates under the action of the precipitant carbon dioxide and the stabilizer organic amine, the precipitates are separated in an inclined plate precipitation tank, the pH value =8 in the inclined plate precipitation tank, the temperature is 24 ℃, the precipitation residence time is 50 minutes, the concentration of the calcium ions of supernatant is 150mg/L, and the concentration of the magnesium ions is 70 mg/L.
S2, pretreating the separated supernatant containing trace carbonate precipitate by an ultrafiltration membrane unit at an operating pressure of 0.25 MPa; then the pure water enters a reverse osmosis membrane unit for concentration, the operation pressure is 2Mpa, the yield of the pure water is more than 85 percent, and the obtained pure water is directly recycled; 9% of concentrated water is generated, the concentrated water is subjected to multi-effect evaporation treatment, and evaporation residues are converted into sludge;
and S3, converting the precipitate obtained in the step S1 into sludge through filter pressing treatment, mixing the sludge with the sludge obtained in the step S2, and transporting the sludge out, wherein the operating pressure of the filter pressing treatment is 0.6Mpa, and the water content of the sludge is 80%.
Comparative example 1
This example is substantially the same as example 7 in which wastewater containing high calcium and magnesium ions and a method for treating wastewater are used, except that: in the step S1, the feed-liquid ratio of the carbon dioxide introduced per unit time to the wastewater is 0.5:1 (mol/L).
As a result: the concentration of calcium ions in the supernatant of S1 was 500mg/L, and the concentration of magnesium ions was 200 mg/L.
Comparative example 2
This example is substantially the same as example 7 in which wastewater containing high calcium and magnesium ions and a method for treating wastewater are used, except that: in step S1, the organic amine is ethylenediamine.
As a result: the concentration of calcium ions in the supernatant of S1 was 400mg/L, and the concentration of magnesium ions was 100 mg/L.
The results from comparative example 1 and comparative example 2 show that: the feed-liquid ratio of the carbon dioxide to the wastewater is less than 0.6:1mol/L, the concentration of calcium and magnesium ions in the supernatant is obviously increased, and the treatment effect is poor; however, the inventor researches and discovers that when the feed-liquid ratio of the carbon dioxide to the wastewater is more than 2.4:1 (mol/L), the effect of removing calcium and magnesium is not obviously improved. When the preferable diethylenetriamine is not used, the concentration of calcium and magnesium ions in the supernatant is also remarkably increased, and the treatment effect is also deteriorated.
The applicant asserts that the present invention is illustrated by the detailed structural features and methods described in the above examples, but the present invention is not limited to the detailed structural features and methods described above, i.e., it is not meant that the present invention must be implemented by relying on the detailed structural features and methods described above. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The implementation of the present invention has been described in detail, however, the present invention is not limited to the specific details of the above-described embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
Claims (6)
1. A zero-emission treatment method for removing calcium and magnesium by using carbon dioxide spray reaction is characterized by comprising the following steps:
s1, converting calcium ions and magnesium ions in wastewater containing high calcium ions and magnesium ions into carbonate precipitates through a carbon dioxide spraying reaction, wherein the total concentration of the calcium ions and the magnesium ions in the wastewater is 10000-12000 mg/L, the feed-liquid ratio of carbon dioxide introduced in unit time to the wastewater is 0.6-2.4: 1 in mol/L, and performing precipitation and separation treatment on a mixture obtained through the spraying reaction;
s2, performing membrane concentration treatment on the separated supernatant containing trace carbonate precipitate, directly recycling the obtained pure water, and performing multi-effect evaporation treatment on the rest concentrated water;
s3, performing filter pressing treatment on the precipitate obtained after the separation treatment to convert the precipitate into sludge, and transporting the sludge outside;
adding organic amine serving as a stabilizer into the wastewater in the step S1, wherein the concentration of the organic amine is 0.01-0.6 mmol/L; the organic amine is diethylenetriamine; the spraying reaction temperature is 5-30 ℃, and the spraying reaction pressure is 0.1-0.5 Mpa.
2. The zero-emission treatment method for removing calcium and magnesium by using carbon dioxide shower reaction according to claim 1, wherein the precipitation conditions in step S1 are as follows: the pH value is 7-8, the temperature is 5-30 ℃, and the deposition retention time is 30-60 min.
3. The zero-emission treatment method for removing calcium and magnesium by using carbon dioxide spray reaction according to claim 1, wherein the membrane concentration treatment in step S2 comprises ultrafiltration pretreatment and reverse osmosis concentration treatment, the operating pressure of the ultrafiltration pretreatment is 0.1-0.3 Mpa, and the operating pressure of the reverse osmosis concentration treatment is 0.9-2.5 Mpa.
4. The zero-emission treatment method for removing calcium and magnesium by using carbon dioxide spray reaction according to claim 1, wherein the operating pressure of the filter pressing treatment in the step S3 is 0.3-0.6 MPa, and the water content of the sludge is 75-80%.
5. The zero-emission treatment method for removing calcium and magnesium by using carbon dioxide spray reaction according to any one of claims 1 to 4, characterized in that a spray reaction tower is used for the spray reaction in step S1, and an inclined plate precipitation unit is used for the precipitation and separation treatment; in the step S2, a membrane concentration unit is adopted in the membrane concentration treatment, and a steam mechanical recompression evaporator is adopted in the multi-effect evaporation treatment; and in the step S3, a plate-and-frame filter press is adopted for filter pressing treatment.
6. A zero discharge treatment system is used for realizing the zero discharge treatment method for removing calcium and magnesium by using carbon dioxide spray reaction as claimed in claim 1, and is characterized by comprising a carbon dioxide spray reaction tower, an inclined plate precipitation unit, a membrane concentration unit, a multi-effect evaporation unit and a filter pressing unit which are connected in sequence.
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| CN1109024A (en) * | 1994-03-19 | 1995-09-27 | 颜寿地 | Method and apparatus for producing lightweight calcium carbonate |
| EP2159197A1 (en) * | 2008-08-25 | 2010-03-03 | Marc Flettner | Method and device for treating water |
| CN103127814A (en) * | 2012-12-24 | 2013-06-05 | 南京大学 | CO2 reaction-absorption integrated device and application thereof for fixing CO2 |
| CN104176857A (en) * | 2014-09-12 | 2014-12-03 | 上海三夫工程技术有限公司 | Treatment technique of manganese-containing wastewater in wet electrolytic manganese production process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109024A (en) * | 1994-03-19 | 1995-09-27 | 颜寿地 | Method and apparatus for producing lightweight calcium carbonate |
| EP2159197A1 (en) * | 2008-08-25 | 2010-03-03 | Marc Flettner | Method and device for treating water |
| CN103127814A (en) * | 2012-12-24 | 2013-06-05 | 南京大学 | CO2 reaction-absorption integrated device and application thereof for fixing CO2 |
| CN104176857A (en) * | 2014-09-12 | 2014-12-03 | 上海三夫工程技术有限公司 | Treatment technique of manganese-containing wastewater in wet electrolytic manganese production process |
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